Reaktionsgleichung
Cl.[CH3:2][NH:3][OH:4].N(C(O[C:11]([CH3:14])([CH3:13])[CH3:12])=O)=[N+]=[N-].[OH-:15].[Na+].[CH3:17]NO.[OH2:20]>>[C:11]([O:15][C:2]([N:3]([CH3:17])[OH:4])=[O:20])([CH3:14])([CH3:13])[CH3:12]Komponenten
Versuchsvorschrift
N-methylhydroxylamine hydrochloride (14.6 g.) in 20 ml. of water was cooled in an ice-bath and treated with 20 g. of t-butyl azidoformate. A solution of 22.4 g. of sodium hydroxide in 80 ml. of water was added dropwise with stirring over 45 minutes while controlling the temperature below 10° C. The mixture was allowed to warm to room temperature with stirring over a 60 minute period after the addition during which time a little more sodium hydroxide solution and N-methyl hydroxylamine were added. The solution was extracted with 2 × 50 ml. of ether, and the extracts were discarded. The aqueous phase, with cooling, was adjusted to pH 3.5 with 6 N hydrochloric acid, and extracted with 5 × 60 ml. of ether. The combined ether extracts were dried over magnesium sulfate and evaporated to 16 g. of oily N-t-butoxycarbonyl-N-methyl hydroxylamine.
Aufarbeitung
- additiontreated with 20 g
- customthe temperature below 10° C
- stirringwith stirring over a 60 minute period
- additionwere added
- extractionThe solution was extracted with 2 × 50 ml
- temperatureThe aqueous phase, with cooling
- extractionextracted with 5 × 60 ml
- dry with materialThe combined ether extracts were dried over magnesium sulfate
- customevaporated to 16 g
Quellen und Nachweise
- ORD-Eintrag
- ord-5342cd172e6b4486a519f99d30ff0ec0
- Quelldatensatz
- uspto-grants-1978_05
- Patentnummer
- US04091105
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